WO2003083157A1 - NITRIDED Mo ALLOY WORKED MATERIAL HAVING HIGH CORROSION RESISTANCE, HIGH STRENGTH AND HIGH TOUGHNESS AND METHOD FOR PRODUCTION THEREOF - Google Patents
NITRIDED Mo ALLOY WORKED MATERIAL HAVING HIGH CORROSION RESISTANCE, HIGH STRENGTH AND HIGH TOUGHNESS AND METHOD FOR PRODUCTION THEREOF Download PDFInfo
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- WO2003083157A1 WO2003083157A1 PCT/JP2003/003912 JP0303912W WO03083157A1 WO 2003083157 A1 WO2003083157 A1 WO 2003083157A1 JP 0303912 W JP0303912 W JP 0303912W WO 03083157 A1 WO03083157 A1 WO 03083157A1
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- Prior art keywords
- alloy
- nitriding
- nitrided
- nitride
- worked material
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/24—Nitriding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
Definitions
- the present invention relates to a nitrided Mo alloy processed material having improved corrosion resistance in addition to strength and toughness by combining internal nitriding and external nitriding, and a method for producing the same.
- Mo has a high melting point of about 260 ° C., has relatively high mechanical strength compared to other high melting point metals, has a low coefficient of thermal expansion, and has good electrical conductivity and good thermal conductivity. It has characteristics such as good corrosion resistance to metal and hydrochloric acid, and has applications such as electrodes, tube parts, semiconductor parts, heat-resistant structural parts, and materials for nuclear reactors.
- the present inventors have previously conducted a multi-stage internal nitridation process to maintain a processed structure on at least the surface side of a processed material of a refractory metal alloy processed material such as Mo in which ultrafine nitride is dispersed and contained. It has been found that high toughness and high strength can be obtained by keeping this state (Patent Document 1, Non-Patent Documents 1-3). Mo has excellent properties as described above, but does not have corrosion resistance to oxidizing acids such as hot concentrated sulfuric acid and nitric acid.
- the present inventors have developed a high corrosion-resistant Mo-based composite material in which a Mo and a Mo-based alloy are subjected to nitriding treatment to provide a Mo 2 N layer having a thickness of 0.5 to 10 ⁇ in (Patent Document 2). ).
- Patent Document 1 JP 2001-73060 A
- Non-Patent Document 1 Masahiro Nagae, Jun Takada, Yoshitoshi Takemoto, Yutaka Hiraoka, Tetsuo Yoshio, Journal of the Japan Institute of Metals, 64 (2000) 747-750
- Non-Patent Document 2 Masahiro Nagae, Jun Takada, Yoshitoshi Takemoto, Yutaka Hiraoka, Tetsuo Yoshio, Journal of the Japan Institute of Metals, 64 (2000) 751-754
- Non-Patent Document 3 Jun Takada, Masahiro Nagae, Yoshitoshi Takemoto, Yutaka Hiraoka, Materia, 40 (2001), 666-667
- Ta metal has been useful as equipment material under ultra-severe corrosion conditions (eg, boiling concentrated sulfuric acid solution).
- Ta metal has low strength, especially at high temperatures, and is not suitable as a structural material for equipment that requires high strength.
- the above high corrosion-resistant Mo-based composite material developed by the present inventors as a material replacing the Ta metal had a disadvantage that the entire material was embrittled as a result of recrystallization of the base material during the manufacturing process.
- the present invention provides sufficiently high corrosion resistance and strength even under ultra-severe corrosion conditions such as a boiling concentrated sulfuric acid solution (eg, 75% H 2 SO 4 aqueous solution (180 ° C)), and furthermore, it can be used at high temperatures.
- the aim is to provide innovative materials with high strength even at low temperatures and high toughness even at low temperatures, combining physical properties not found in conventional materials, and efficient production methods for them.
- Mo alloys have high strength, high toughness and excellent corrosion resistance to oxidizing acids at low cost. It has been found that a processed material can be obtained.
- the fine nitride generated by internally nitriding the nitride-forming metal element dissolved in the Mo alloy processing material is dispersed therein, and further, the processed tissue or the recovery structure on the surface of the processed material is externally formed.
- This is a highly corrosion-resistant, high-strength, high-toughness nitrided Mo alloy processed material characterized by having a Mo nitride layer formed on the surface formed by nitriding.
- the present invention provides the above-mentioned nitriding-treated Mo alloy processing material, wherein the Mo nitride on the surface of the processing material is at least one of ⁇ - ⁇ , ⁇ -M02N or / 3-3 ⁇ 2 2. is there.
- the present invention is the above-mentioned nitrided Mo alloy processed material, wherein the layer between the Mo nitride layer and the parent phase inside the processed material has a processed structure or a recovered structure. Further, the present invention is the above-mentioned nitrided Mo alloy base material, wherein the inside of the alloy has a recrystallized structure.
- the processing temperature is increased stepwise to an alloy processing material in which at least one of Ti, Zr, Hf, V, Nb, and Ta is used as a solid phase with Mo as a mother phase. 5.
- FIG. 1 is a schematic view showing a cross-sectional structure of a nitrided Mo alloy processed material of the present invention.
- FIG. 2 is a schematic diagram showing the structure of the processed material at each stage of the internal nitriding processes (1) to (3) in the process of producing the nitrided Mo alloy processed material of the present invention.
- FIG. 3 is a graph showing the corrosion test results of the nitrided Mo alloy processed material obtained in Example 1 and Example 2 and the comparative example (pure Mo material). Fig.
- Example 4 is a photograph of a cross-sectional structure of a nitrified Mo alloy processed material obtained in Example 2 as a substitute for a drawing (a) and a macro photograph of a nitrified Mo alloy processed material specimen after a bending test (b). It is. BEST MODE FOR CARRYING OUT THE INVENTION
- FIG. 1 is a schematic diagram showing an example of a cross-sectional structure of a nitrided Mo alloy processed material of the present invention.
- FIG. 1 shows a nitrided Mo alloy processed material according to the present invention. It has a three-layer structure including the Mo 2 N surface layer 4 formed by nitriding and the Mo recrystallized layer 5 inside the processed material. If the work material is relatively thin, it is possible to keep the texture completely inside, in which case a two-layer structure without the Mo recrystallized layer 5 is obtained.
- the work material is a material obtained by subjecting a dilute alloy in which at least one of Ti, Zr, Hf, V, Nb, and Ta is dissolved to a solid phase with Mo as a mother phase, such as rolling.
- a dilute alloy is an alloy that contains a small amount of solute elements in solid solution alloys of about 5% by weight or less.
- the high corrosion resistance, high strength, and high toughness nitriding treatment of the present invention is manufactured by the following internal nitriding treatments (1) to (3) and external nitriding treatment (4).
- (3) is a schematic diagram showing the structure of the processed material at each stage of the internal nitriding treatments (1) to (3) performed by gradually increasing the treatment temperature.
- First-stage nitriding treatment Heating in a nitriding atmosphere at a temperature lower than the upper limit of recrystallization and at a temperature higher than the lower limit of recrystallization of 200 ° C. The oxide particles are dispersed and formed.
- nitrogen is diffused into the work material while maintaining the work structure X1 of the dilute alloy work material, thereby preferentially nitriding the nitride-forming metal element that is dissolved in the parent phase to obtain a diameter 1
- Sub-nano-plate-like nitride particles of about 2 nm are formed and dispersed in the matrix.
- preferential nitriding refers to a phenomenon in which only a nitride-forming element, not a metal in a parent phase, is preferentially nitrided.
- the recrystallization temperature of the surface of the work material increases due to the pinning effect of the precipitated particles generated by this nitriding treatment. .
- Second-stage nitriding The workpiece obtained by the first-stage nitriding is heated in a nitriding atmosphere at a temperature equal to or higher than the recrystallization lower limit temperature to grow and stabilize ultrafine nitride particles.
- the recrystallization temperature further increases due to the growth and stabilization of precipitated particles by the second-stage nitriding treatment.
- the inside of the work material is recrystallized and the work structure X2 remains, but when the work material is relatively thin (3 mm or less), the work structure can be completely retained inside.
- rod-shaped nitride particles of about 10 nm in thickness and about 50 nm in length are uniformly dispersed in the Mo matrix.
- the third and subsequent stages, such as the fourth and fifth stages The processing can be appropriately performed.
- a strong nitride treatment forms a Mo nitride layer on the surface.
- the formed Mo nitride comprises at least one of ⁇ - ⁇ , ⁇ -Mo 2 Mo or] 3—Mo 2 ⁇ .
- a processed or recovered structure is left between the Mo nitride surface layer and the parent phase inside the processed material.
- Table 1 shows the relationship between the heat treatment temperature of the external nitriding treatment and the film thickness for the case of Mo-0.5wt% Ti alloy.
- the higher the heating temperature the larger the film thickness. From the viewpoint of corrosion resistance, it can be said that the thicker the film, the better. However, it was found that as the thickness increases, the transversibility (bending property) decreases. Therefore, as a condition that combines toughness and corrosion resistance, it is necessary to use an external nitriding treatment (thickness of about 3 mm or less) at 900 ° C or less. (table 1)
- the nitrided Mo alloy processed material of the present invention is a semiconductor 'ceramics' metal high-temperature firing support plate, a high-temperature heating furnace heater, a high-temperature heating furnace member, and a chemical equipment and equipment structure used in a corrosive environment.
- Materials including high-temperature incinerators, etc.), supercritical and subcritical solution reactor materials, acid-resistant containers and tubes for oxidizing acids such as sulfuric acid and nitric acid, and extreme severe corrosion conditions It is useful as an equipment material below (for example, boiling sulfuric acid concentrated sulfuric acid solution), an ultra-high temperature heater, a metal injection mold, and a spray nozzle for diesel engines.
- the surface area of the processed material retains the processed and recovered structure (the recrystallized structure inside), and also diffuses and precipitates fine TIN particles.
- an external nitride treatment is performed at 1000 ° C for 4 hours in a stream of NH 3 gas (1 atm) to form a 14. ⁇ thick Mo nitride (y-Mo 2 N, etc.) layer on the surface of the processed material. did.
- the surface of the processed material is a Mo nitride layer
- the inner side is a nitride layer of a solid solution element having Mo as a mother phase in a processed / recovered grain structure in which fine TiN particles are dispersed and precipitated.
- the inside has a three-layer structure of a Mo alloy layer with a large equiaxed recrystallized grain structure.
- Fig. 3 shows the results of a corrosion test conducted in a 75% concentrated sulfuric acid boiling solution (185 ° C) in order to examine the corrosion resistance in a severely corrosive environment.
- Fig. 3 also shows the result of pure Mo as a comparative sample.
- the corrosion rate of pure Mo is as high as 8 mm / year, and corrodes violently, whereas the processed material of the present invention hardly corrodes at 0.076 mmZ (Example 1) and has almost perfect corrosion resistance (corrosion resistance). (Speed: 0.05 mmZ).
- Example 2 shows the results of a corrosion test conducted in a 75% concentrated sulfuric acid boiling solution
- Heating temperature of Mo-0.5wt% Ti alloy material in N2 gas (1 atm) was changed to three-stage internal nitriding.
- the temperature was 900 ° C ⁇ 1200 ° C ⁇ 1500 ° C.
- the three-stage internally nitrided Mo alloy is further heated (external nitridation) at 900 ° C for 4 hours in a 1 atm NH 3 gas stream, and Mo nitride ( ⁇ - ⁇ , ⁇ -Mo 2N )
- the layer was formed uniformly.
- Figure 3 shows the results of a corrosion test performed in a 75% concentrated sulfuric acid boiling solution (185 ° C).
- the processed material of Example 2 hardly corrodes at 0.46 mm / year and shows complete corrosion resistance (corrosion rate: 0.05 mm / year).
- Fig. 4 shows (a) a photograph of the cross-sectional structure and (b) a macro photograph of the specimen after the bending test.
- the present invention provides a nitriding treated Mo alloy material that has high strength, high toughness, excellent corrosion resistance against oxidizing acids, and can be used in extremely corrosive environments, efficiently and inexpensively only by nitriding.
- equipment materials under ultra-severe corrosive conditions eg, boiling concentrated sulfuric acid solution
- ultra-high temperature heaters e.g., boiling concentrated sulfuric acid solution
- metal injection molds e.g., diesel engine molds
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
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- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
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Abstract
Description
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Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA002480787A CA2480787A1 (en) | 2002-03-29 | 2003-03-27 | Nitrided mo alloy worked material having high corrosion resistance, high strength and high toughness and method for production thereof |
AT03745433T ATE533870T1 (en) | 2002-03-29 | 2003-03-27 | NITRIDATED MO ALLOY MATERIAL WITH HIGH CORROSION RESISTANCE, HIGH STRENGTH AND HIGH TOUGHNESS AND PRODUCTION PROCESS THEREOF |
EP03745433A EP1491651B1 (en) | 2002-03-29 | 2003-03-27 | NITRIDED Mo ALLOY WORKED MATERIAL HAVING HIGH CORROSION RESISTANCE, HIGH STRENGTH AND HIGH TOUGHNESS AND METHOD FOR PRODUCTION THEREOF |
US10/509,156 US20060054247A1 (en) | 2002-03-29 | 2003-03-27 | Nitrided mo alloy worked material having high corrosion resistance, high strength and high toughness and method for production thereof |
KR1020047015093A KR100611725B1 (en) | 2002-03-29 | 2003-03-27 | Nitrided Mo alloy worked material having high corrosion resistance, high strenth and high toughness and method for prodution thereof |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2002-98039 | 2002-03-29 | ||
JP2002098039A JP4302930B2 (en) | 2002-03-29 | 2002-03-29 | High corrosion resistance, high strength, high toughness Nitrided Mo alloy processed material and its manufacturing method |
Publications (1)
Publication Number | Publication Date |
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WO2003083157A1 true WO2003083157A1 (en) | 2003-10-09 |
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ID=28671934
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PCT/JP2003/003912 WO2003083157A1 (en) | 2002-03-29 | 2003-03-27 | NITRIDED Mo ALLOY WORKED MATERIAL HAVING HIGH CORROSION RESISTANCE, HIGH STRENGTH AND HIGH TOUGHNESS AND METHOD FOR PRODUCTION THEREOF |
Country Status (7)
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US (1) | US20060054247A1 (en) |
EP (1) | EP1491651B1 (en) |
JP (1) | JP4302930B2 (en) |
KR (1) | KR100611725B1 (en) |
AT (1) | ATE533870T1 (en) |
CA (1) | CA2480787A1 (en) |
WO (1) | WO2003083157A1 (en) |
Families Citing this family (6)
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JP4255877B2 (en) * | 2004-04-30 | 2009-04-15 | 株式会社アライドマテリアル | High-strength and high recrystallization temperature refractory metal alloy material and its manufacturing method |
JP4558572B2 (en) * | 2005-04-25 | 2010-10-06 | 株式会社アライドマテリアル | High heat resistant molybdenum alloy and manufacturing method thereof |
CN103409718B (en) * | 2013-05-15 | 2015-08-26 | 厦门虹鹭钨钼工业有限公司 | A kind of High-temperature oxidation-resistant molybdenum material and production method thereof |
CN106535826A (en) | 2014-06-24 | 2017-03-22 | 怡康医疗股份有限公司 | Improved metal alloys for medical devices |
US10682437B2 (en) | 2015-07-02 | 2020-06-16 | Mirus Llc | Molybdenum alloys for medical devices |
WO2017151548A1 (en) | 2016-03-04 | 2017-09-08 | Mirus Llc | Stent device for spinal fusion |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS59208066A (en) * | 1983-05-13 | 1984-11-26 | Toshiba Corp | Method for working internally nitrided molybdenum-zirconium alloy |
JPH11286770A (en) | 1998-04-01 | 1999-10-19 | Yoshioka Takashi | High corrosion resistance molybdenum-based composite material and its production |
WO2001018276A1 (en) | 1999-09-06 | 2001-03-15 | Japan Science And Technology Corporation | High melting point metal based alloy material having high toughness and strength |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SU1747535A1 (en) * | 1990-07-29 | 1992-07-15 | Научно-исследовательский физико-химический институт им.Л.Я.Карпова | Method of molybdenum nitriding |
-
2002
- 2002-03-29 JP JP2002098039A patent/JP4302930B2/en not_active Expired - Fee Related
-
2003
- 2003-03-27 CA CA002480787A patent/CA2480787A1/en not_active Abandoned
- 2003-03-27 KR KR1020047015093A patent/KR100611725B1/en not_active IP Right Cessation
- 2003-03-27 EP EP03745433A patent/EP1491651B1/en not_active Expired - Fee Related
- 2003-03-27 AT AT03745433T patent/ATE533870T1/en active
- 2003-03-27 WO PCT/JP2003/003912 patent/WO2003083157A1/en active Application Filing
- 2003-03-27 US US10/509,156 patent/US20060054247A1/en not_active Abandoned
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS59208066A (en) * | 1983-05-13 | 1984-11-26 | Toshiba Corp | Method for working internally nitrided molybdenum-zirconium alloy |
JPH11286770A (en) | 1998-04-01 | 1999-10-19 | Yoshioka Takashi | High corrosion resistance molybdenum-based composite material and its production |
WO2001018276A1 (en) | 1999-09-06 | 2001-03-15 | Japan Science And Technology Corporation | High melting point metal based alloy material having high toughness and strength |
JP2001073060A (en) | 1999-09-06 | 2001-03-21 | Japan Science & Technology Corp | High melting point metallic alloy material having high toughness and high strength |
Non-Patent Citations (4)
Title |
---|
MASAHIRO NAGAE ET AL., NITRIDING OF DILUTE MO-TI ALLOYS AT LOW TEMPERATURE OF 1373K, 1998, pages 127 - 132 |
MASAHIRO NAGAE; JUN TAKADA; YOSHITO TAKEMOTO; YUTAKA HIRAOKA; TETSUO YOSHIO., J. JAPAN INST. METALS, vol. 64, 2000, pages 747 - 750 |
MASAHIRO NAGAE; JUN TAKADA; YUTAKA HIRAOKA; YOSHITO TAKEMOTO, MATERIA JAPAN, vol. 40, 2001, pages 666 - 667 |
MASAHIRO NAGAE; JUN TAKADA; YUTAKA HIRAOKA; YOSHITO TAKEMOTO; TETSUO YOSHIO., J. JAPAN INST. METALS, vol. 64, 2000, pages 751 - 754 |
Also Published As
Publication number | Publication date |
---|---|
ATE533870T1 (en) | 2011-12-15 |
EP1491651A4 (en) | 2008-08-27 |
KR20040105796A (en) | 2004-12-16 |
CA2480787A1 (en) | 2003-10-09 |
EP1491651A1 (en) | 2004-12-29 |
JP4302930B2 (en) | 2009-07-29 |
EP1491651B1 (en) | 2011-11-16 |
KR100611725B1 (en) | 2006-08-10 |
JP2003293116A (en) | 2003-10-15 |
US20060054247A1 (en) | 2006-03-16 |
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